CN115594513B - In-situ generated carbon fiber reinforced silicon carbide ceramic matrix composite material and preparation method thereof - Google Patents

In-situ generated carbon fiber reinforced silicon carbide ceramic matrix composite material and preparation method thereof Download PDF

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CN115594513B
CN115594513B CN202211271308.0A CN202211271308A CN115594513B CN 115594513 B CN115594513 B CN 115594513B CN 202211271308 A CN202211271308 A CN 202211271308A CN 115594513 B CN115594513 B CN 115594513B
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carbon fiber
silicon carbide
matrix composite
ceramic matrix
carbide ceramic
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CN115594513A (en
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陈毛
陈勇强
范冰冰
王海龙
刘慧�
耿文钊
邵刚
张锐
李红霞
方成
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Zhengzhou University
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Abstract

The invention discloses an in-situ generated carbon fiber reinforced silicon carbide ceramic matrix composite material and a preparation method thereof, and belongs to the field of ceramic microwave sintering. The preparation method comprises the following steps: 1) Ball milling and mixing SiC powder, a sintering aid, a binder and a catalyst to obtain a mixture; 2) Pressing and forming the mixture to obtain a green body; 3) And (3) sintering the green blank in a segmented manner to prepare the carbon fiber reinforced silicon carbide ceramic matrix composite. The carbon fiber reinforced silicon carbide ceramic matrix composite obtained by the preparation method has the advantages of high volume density, high flexural strength, short preparation period, low sintering temperature, controllable carbon fiber diameter and capability of being prepared from nano-scale to micro-scale; the preparation process is simple, the prefabricated body can be prepared without using carbon fiber, the preparation can be completed by one-time sintering, the applicability is wide, the operation is convenient, the method is suitable for industrialized rapid production, and the method has wide application prospect.

Description

In-situ generated carbon fiber reinforced silicon carbide ceramic matrix composite material and preparation method thereof
Technical Field
The invention belongs to the technical field of ceramics, and particularly relates to an in-situ generated carbon fiber reinforced silicon carbide ceramic matrix composite material and a preparation method thereof.
Background
The carbon fiber reinforced silicon carbide (C/SiC) ceramic matrix composite material fully utilizes the excellent high-temperature mechanical property of carbon fiber and the high-temperature oxidation resistance of a SiC ceramic matrix, has low density, high strength and excellent thermal stability and chemical stability, is considered as the most promising high-temperature structural material at present, and has been successfully applied to the fields of aerospace, military industry, civil industry and the like.
The existing preparation methods of the carbon fiber reinforced silicon carbide (C/SiC) ceramic matrix composite material mainly comprise a chemical vapor infiltration method (CVI), a reactive melt infiltration method (RMI), a slurry impregnation hot pressing method (SIHP), a precursor impregnation pyrolysis method (PIP), a chemical liquid vapor deposition method (CLVD), a composite method of the processes and the like. These methods are all to prepare a carbon fiber preform first, and then introduce a silicon carbide matrix into the carbon fiber preform to form a dense composite material.
The main advantages of Chemical Vapor Infiltration (CVI) include relatively low processing temperatures, low fiber damage, high matrix purity, and the ability to produce parts of complex shape; its main disadvantages are high residual porosity (up to 10% -15%), long preparing time and high cost.
The advantages of Precursor Impregnation Pyrolysis (PIP) are mainly: the process is simple, the penetration depth is large, the prepared SiC matrix is uniform, the processing temperature is relatively low, the damage to carbon fibers is small, the composition of the matrix can be controlled, the preparation of complex components can be realized, and compared with a CVI method, the method is more economical. However, the composite material prepared by the PIP method has long process period, high porosity, large volume deformation and low production efficiency, and is unfavorable for production and application.
The Reactive Melt Infiltration (RMI) method has the advantages of short preparation time, high density, low cost, capability of preparing components with complex shapes and the like, but residual Si is easy to leave in a matrix, the residual Si reacts with carbon fibers to damage the fibers, and the oxidation resistance and mechanical properties of the composite material are reduced.
The slurry impregnation hot pressing method (SIHP) has the advantages of simple process, low porosity, low cost and close to net size molding, but the method has the defects that powder particles in the slurry are easy to agglomerate to block pores of the outer layer of the fiber preform, and the fiber is easy to damage under the high-temperature and high-pressure sintering condition, so that the method is not suitable for preparing complex structural members.
The chemical vapor deposition (CLVD) can avoid the phenomenon of surface crusting which is frequently generated in the traditional chemical vapor infiltration method, the densification effect is good, the composition structure of the matrix can be designed, and the deposition rate is about 2 orders of magnitude higher than that of the chemical vapor infiltration method. The process has the disadvantages that the prefabricated body with larger shape and size needs induction coils and heating bodies with different sizes, the radius of the prefabricated body is large enough to generate a certain thermal gradient, and the equipment is ensured to provide larger power.
The production process is complex in steps, high in equipment requirement, high in energy consumption and not in accordance with the green development requirement, and some pollutants are discharged in the production process.
Disclosure of Invention
The invention aims to provide an in-situ generated carbon fiber reinforced silicon carbide ceramic matrix composite material and a preparation method thereof, which can realize the efficient green preparation of the composite material and solve the problems of complex process, long production period, high sintering temperature, serious pollution and high energy consumption in the preparation of the carbon fiber reinforced silicon carbide ceramic matrix composite material by the existing preparation method.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of an in-situ generated carbon fiber reinforced silicon carbide ceramic matrix composite, which comprises the following steps:
1) Ball milling and mixing SiC powder, a sintering aid, a binder and a catalyst to obtain a mixture;
2) Pressing and forming the mixture to obtain a green body;
3) And (3) sintering the green blank in a segmented manner to prepare the carbon fiber reinforced silicon carbide ceramic matrix composite.
Preferably, the sintering aid comprises SiO 2 、MgO、Al 2 O 3 And Y 2 O 3 Any one or more of the following; the binder comprises a polymer comprising polyethylene glycol, ethanol, polyvinyl alcohol, and carboxymethyl celluloseAny one or more of vitamins; the catalyst comprises Fe/Ni alloy powder.
Preferably, in the Fe/Ni alloy powder, the mass ratio of Fe to Ni is 5:0.5 to 1.
Preferably, the mass ratio of the SiC powder to the sintering aid to the binder to the catalyst is 90-98: 1 to 5:0.5 to 3:1 to 3.
Preferably, the particle size of the SiC powder is 80-120 meshes.
Preferably, the ball milling condition in the step 1) is that the ball-to-material ratio is 1: 2-5, the rotating speed is 100-300 r/min, and the ball milling time is 180-300 min.
Preferably, the molding pressure in the step 2) is 80-120 Mpa, and the dwell time is 1-5 min.
Preferably, the step 3) of the staged sintering comprises the following two stages: the first stage is to heat to 1000-1200 ℃ at a heating rate of 3-5 ℃/min, and keep the temperature for 0.5-2 h; the second stage heats to 1400-1600 ℃ at a heating rate of 3-5 ℃/min, and keeps the temperature for 1-3 h.
Preferably, the environment of the step 3) is a vacuum environment, and the vacuum degree is 5-20 Pa.
The invention also aims to provide an in-situ generated carbon fiber reinforced silicon carbide ceramic matrix composite material prepared by the preparation method.
Compared with the prior art, the invention has the following beneficial effects:
the preparation method of the in-situ generated carbon fiber reinforced silicon carbide ceramic matrix composite material can be completed by one-time sintering, carbon fibers can be generated in situ at the temperature of 1000-1200 ℃ after the blank is pressed and molded, steam volatilization can be formed by the metal catalyst along with the increase of the sintering temperature, and meanwhile, densification of a SiC matrix is realized under the action of a sintering aid.
The invention relates to a preparation method of an in-situ generated carbon fiber reinforced silicon carbide ceramic matrix composite, which comprises the steps of putting a pressed green body into a vacuum furnace, and sintering by adopting two-stage heating in a vacuum environment. In the first stage, under the action of a catalyst, partial silicon carbide is decomposed to generate carbon fibers in situThe problem that the carbon fiber preform prepared by the conventional process is easy to damage is avoided, and the generated carbon fiber has a good contact interface with SiC, so that the strength and toughness of the material are further improved. And the number and the diameter of the carbon fibers generated in situ can be controlled by a process, and the carbon fibers with different morphologies can be obtained by adjusting the addition amount of the catalyst and the heat preservation time. The second stage is heated to 1400-1600 ℃ for heat preservation, different temperatures are selected according to different sintering aids, the SiC matrix is densified rapidly in the second stage, defects generated in the reaction process of the first stage are improved obviously, and the final performance of the material is improved. The volume density of the carbon fiber reinforced silicon carbide ceramic matrix composite obtained by the process is 2.98g/cm 3 The flexural strength is 532MPa, the preparation period is short, the sintering temperature is low, the diameter of the carbon fiber is controllable, and the carbon fiber can be prepared from nano-scale to micro-scale; the preparation process is simple, the prefabricated body can be prepared without using carbon fiber, the applicability is wide, the operation is convenient, the method is suitable for industrialized rapid production, no pollution is discharged in the material preparation and sintering process, the sintering temperature is low, the time is short, the energy consumption is low, and the method has wide application prospect.
Drawings
FIG. 1 is a SEM image of a fracture of a carbon fiber reinforced silicon carbide ceramic matrix composite obtained in example 1;
FIG. 2 is an SEM image of a carbon fiber reinforced silicon carbide ceramic matrix composite obtained in example 3;
FIG. 3 is a SEM image of a carbon fiber-reinforced silicon carbide ceramic matrix composite obtained in example 3;
FIG. 4 is a TEM image (100 nm) of carbon fibers in the carbon fiber-reinforced silicon carbide ceramic matrix composite obtained in example 1.
FIG. 5 is a TEM image (50 nm) of carbon fibers in the carbon fiber-reinforced silicon carbide ceramic matrix composite obtained in example 1.
Detailed Description
The invention provides a preparation method of an in-situ generated carbon fiber reinforced silicon carbide ceramic matrix composite, which comprises the following steps:
1) Ball milling and mixing SiC powder, a sintering aid, a binder and a catalyst to obtain a mixture;
2) Pressing and forming the mixture to obtain a green body;
3) And (3) sintering the green blank in a segmented manner to prepare the carbon fiber reinforced silicon carbide ceramic matrix composite.
In the present invention, the sintering aid comprises SiO 2 、MgO、Al 2 O 3 And Y 2 O 3 Any one or more of the following; the binder comprises any one or more of polyethylene glycol, ethanol, polyvinyl alcohol and carboxymethyl cellulose; the catalyst is preferably Fe/Ni alloy powder.
In the invention, in the Fe/Ni alloy powder, the mass ratio of Fe to Ni is preferably 5:0.5 to 1, more preferably 5:0.6 to 0.9, still more preferably 5:0.8.
In the invention, the mass ratio of the SiC powder, the sintering aid, the binder and the catalyst is preferably as follows: 90-98: 1 to 5:0.5 to 3:1 to 3, more preferably 93 to 97:2 to 5:0.5 to 2:1 to 2.5, more preferably 93 to 95:2 to 4:1 to 1.5:1.5 to 2.
In the present invention, the particle size of the SiC powder is preferably 80 to 120 mesh, preferably 90 to 110 mesh, more preferably 100 mesh.
In the present invention, the ball milling conditions in step 1) are that the ball-to-material ratio is preferably 1:2 to 5, more preferably 1:2 to 4, more preferably 1:2.5 to 3.5; the rotation speed is preferably 100 to 300r/min, more preferably 150 to 300r/min, and still more preferably 200 to 300r/min; the ball milling time is preferably 180 to 300 minutes, more preferably 200 to 300 minutes, and still more preferably 240 to 280 minutes.
In the present invention, the molding pressure in the step 2) is preferably 80 to 120Mpa, more preferably 90 to 110Mpa, still more preferably 95 to 100Mpa; the dwell time is preferably 1 to 5 minutes, more preferably 1.5 to 4 minutes, and still more preferably 2 to 3 minutes.
In the present invention, the staged sintering described in step 3) comprises two stages.
In the present invention, the temperature rising rate in the first stage is preferably 3 to 5℃per minute, more preferably 4 to 5℃per minute, still more preferably 4℃per minute; preferably, the temperature is raised to 1000 to 1200 ℃, more preferably 1050 to 1150 ℃, and even more preferably 1100 to 1150 ℃; the holding time is preferably 0.5 to 2 hours, more preferably 1 to 1.5 hours, and still more preferably 1 to 1.2 hours.
In the present invention, the temperature rising rate in the second stage is preferably 3 to 5℃per minute, more preferably 4 to 5℃per minute, still more preferably 4℃per minute; preferably, the temperature is raised to 1400-1600 ℃, more preferably 1450-1550 ℃, and still more preferably 1500-1550 ℃; the holding time is preferably 1 to 3 hours, more preferably 1.5 to 2.5 hours, and still more preferably 1.5 to 2 hours.
In the present invention, the atmosphere for the stage sintering in step 3) is a vacuum atmosphere, and the vacuum degree is preferably 5 to 20Pa, more preferably 8 to 15Pa, and still more preferably 10Pa.
In the present invention, the carbon fibers are generated in situ during sintering, and the carbon fibers are not required to be used for preparing the preform.
In the invention, the diameter of the carbon fiber generated in situ in the sintering process is controllable within the range of 10nm-16 mu m, and can be adjusted according to the requirements of the applicable scene of the material.
The technical solutions provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
1) 97g of SiC powder (particle size 80 meshes) and SiO 2 3g, 2g of glycol and 3g of Fe/Ni catalyst (the ratio of Fe/Ni is 5:0.5), and ball milling and mixing are carried out, wherein the ball-material ratio is 1:5, the rotating speed is 300r/min, and the ball milling time is 300min; and (3) pressing and forming the mixture by using a tablet press, wherein the forming pressure is 120Mpa, and the pressure maintaining time is 1min. The method comprises the steps of carrying out a first treatment on the surface of the
2) Placing the pressed green blanks into a vacuum furnace, vacuumizing to 10Pa, heating from room temperature to 1000 ℃ at the speed of 3 ℃/min, preserving heat for 0.5h, heating to the sintering temperature of 1400 ℃ at the speed of 3 ℃/min, preserving heat for 1h, turning off a power supply, and naturally cooling to the room temperature to obtain the carbon fiber reinforced silicon carbide ceramic matrix composite.
The results obtained in this exampleThe diameter of the carbon fiber reinforced silicon carbide ceramic matrix composite is 20nm, and the volume density is 3.02g/cm 3 The flexural strength is 502MPa.
Fig. 1 is an SEM image of a fracture of the carbon fiber reinforced silicon carbide ceramic matrix composite obtained in example 1, in which the generated carbon fiber is observed, and some holes exist in the fracture, so that the SiC ceramic is converted from a traditional brittle fracture to a ductile fracture by the existence of the carbon fiber, and the fracture becomes staggered, so that the breaking strength of the SiC composite ceramic can be remarkably improved. Fig. 4 and 5 are TEM images of carbon fibers in the carbon fiber reinforced silicon carbide ceramic matrix composite obtained in example 1, and it can be seen from the figures that the diameter of the produced carbon fibers is about 100nm, and the diameter of the carbon fibers is controllable.
Example 2
The preparation method of the in-situ generated carbon fiber reinforced silicon carbide ceramic matrix composite material comprises the following steps:
1) 95g of SiC powder (particle size 80 meshes) and Al are taken 2 O 3 5. 5g, ethanol 2g and Fe/Ni catalyst 2.5g (Fe/Ni ratio is 5:1), ball milling and mixing, ball material ratio is 1:4, the rotating speed is 280r/min, and the ball milling time is 270min; and (3) pressing and forming the mixture by using a tablet press, wherein the forming pressure is 110Mpa, and the pressure maintaining time is 2min.
2) Placing the pressed green blanks into a vacuum furnace, vacuumizing to 10Pa, heating from room temperature to 1000 ℃ at the speed of 3 ℃/min, preserving heat for 1h, heating to the sintering temperature of 1450 ℃ at the speed of 3 ℃/min, preserving heat for 2h, closing a power supply, and naturally cooling to the room temperature to obtain the carbon fiber reinforced silicon carbide ceramic matrix composite.
The carbon fiber-reinforced silicon carbide ceramic matrix composite obtained in this example has a carbon fiber diameter of 100nm and a bulk density of 2.99g/cm 3 The flexural strength is 516MPa.
Example 3
The preparation method of the in-situ generated carbon fiber reinforced silicon carbide ceramic matrix composite material comprises the following steps:
1) 96g of SiC powder (particle size 100 mesh), 4g of MgO, 3g of ethylene glycol and 2g of Fe/Ni catalyst (the proportion of Fe/Ni is 5: 1) Ball milling and mixing are carried out, and the ball-material ratio is 1:3, the rotating speed is 250r/min, and the ball milling time is 240min; and (3) pressing and forming the mixture by a tablet press, wherein the forming pressure is 100Mpa, and the pressure maintaining time is 3min.
2) Placing the pressed green blanks into a vacuum furnace, vacuumizing to 5Pa, heating from room temperature to 1100 ℃ at a speed of 3 ℃/min, preserving heat for 1h, then heating to a sintering temperature of 1480 ℃ at a speed of 3 ℃/min, preserving heat for 2.5h, turning off a power supply, and naturally cooling to room temperature to obtain the carbon fiber reinforced silicon carbide ceramic matrix composite.
The carbon fiber-reinforced silicon carbide ceramic matrix composite obtained in this example has a carbon fiber diameter of 10 μm and a bulk density of 2.98g/cm 3 The flexural strength is 532MPa.
FIG. 2 is an SEM image of a carbon fiber reinforced silicon carbide ceramic matrix composite obtained in example 3, in which it can be seen that the SiC matrix has carbon fibers distributed therein, the interface contact between the two is good, and the matrix is relatively dense; fig. 3 is a carbon fiber SEM image of the carbon fiber reinforced silicon carbide ceramic matrix composite obtained in example 3, under which the carbon fiber may have a diameter as long as ten micrometers.
Example 4
1) 94g of SiC powder (particle size 100 meshes) and Al are taken 2 O 3 /Y 2 O 3 2g of mixture (Al 2 O 3 /Y 2 O 3 The ratio of (2) is 10: 1) 3g of carboxymethyl cellulose and 1.5g of Fe/Ni catalyst (the proportion of Fe/Ni is 5:1), and ball milling and mixing are carried out, wherein the ball-material ratio is 1:2; the rotating speed is 200r/min, and the ball milling time is 210min; and (3) pressing and forming the mixture by using a tablet press, wherein the forming pressure is 90Mpa, and the pressure maintaining time is 4min.
2) Placing the pressed green blanks into a vacuum furnace, vacuumizing to 10Pa, heating from room temperature to 1100 ℃ at a speed of 3 ℃/min, preserving heat for 1.2h, heating to a sintering temperature of 1500 ℃ at a speed of 3 ℃/min, preserving heat for 1.5h, turning off a power supply, and naturally cooling to room temperature to obtain the carbon fiber reinforced silicon carbide ceramic matrix composite.
The carbon fiber reinforced silicon carbide ceramic obtained in the embodimentThe diameter of the carbon fiber of the ceramic matrix composite is 12 mu m, and the volume density is 2.78g/cm 3 The flexural strength is 523MPa.
Example 5
1) 95g of SiC powder (particle size of 110 meshes) and MgO/Y are taken 2 O 3 5g of mixture (MgO/Y) 2 O 3 The ratio of (2) is 5: 1) 3g of polyvinyl alcohol and 1g of Fe/Ni catalyst (the proportion of Fe/Ni is 5:1), and performing ball milling mixing, wherein the ball-material ratio is 1:3; the rotating speed is 150r/min, and the ball milling time is 180min; and (3) pressing and forming the mixture by a tablet press, wherein the forming pressure is 100Mpa, and the pressure maintaining time is 3min.
2) Placing the pressed green blanks into a vacuum furnace, vacuumizing to 15Pa, heating from room temperature to 1200 ℃ at the speed of 4 ℃/min, preserving heat for 2h, heating to the sintering temperature of 1540 ℃ at the speed of 4 ℃/min, preserving heat for 3h, closing a power supply, and naturally cooling to the room temperature to obtain the carbon fiber reinforced silicon carbide ceramic matrix composite.
The carbon fiber-reinforced silicon carbide ceramic matrix composite obtained in this example had a carbon fiber diameter of 16 μm and a bulk density of 2.73g/cm 3 The flexural strength is 486MPa.
Example 6
1) 98g of SiC powder (particle size of 120 meshes) and Al are taken 2 O 3 /MgO/Y 2 O 3 5g of mixture (Al) 2 O 3 /MgO/Y 2 O 3 The ratio of (2) is 4:4: 1) Carboxymethyl cellulose/ethanol 3g (carboxymethyl cellulose/ethanol ratio 1: 9) 1.5g of Fe/Ni catalyst (the proportion of Fe/Ni is 5:0.8), and ball milling and mixing are carried out, wherein the ball-material ratio is 1:3; the rotating speed is 100r/min, and the ball milling time is 240min; and (3) pressing and forming the mixture by a tablet press, wherein the forming pressure is 100Mpa, and the pressure maintaining time is 3min.
2) And (3) placing the pressed green blanks into a vacuum furnace, vacuumizing to 20Pa, heating from room temperature to 1100 ℃ at a speed of 5 ℃/min, preserving heat for 1.5 hours, heating to a sintering temperature of 1600 ℃ at a speed of 5 ℃/min, preserving heat for 2 hours, turning off a power supply, and naturally cooling to room temperature to obtain the carbon fiber reinforced silicon carbide ceramic matrix composite.
As in the present embodimentThe diameter of the carbon fiber of the obtained carbon fiber reinforced silicon carbide ceramic matrix composite is 10 mu m, and the volume density is 2.97g/cm 3 The flexural strength is 518MPa.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.

Claims (8)

1. The preparation method of the in-situ generated carbon fiber reinforced silicon carbide ceramic matrix composite material is characterized by comprising the following steps of:
1) Ball milling and mixing SiC powder, a sintering aid, a binder and a catalyst to obtain a mixture;
2) Pressing and forming the mixture to obtain a green body;
3) The green body is sintered in sections to prepare the carbon fiber reinforced silicon carbide ceramic matrix composite;
the catalyst comprises Fe/Ni alloy powder; in the Fe/Ni alloy powder, the mass ratio of Fe to Ni is 5:0.5-1;
the step 3) of the segmented sintering comprises the following two stages: the first stage is to heat to 1000-1200 ℃ at a heating rate of 3-5 ℃/min, and keep the temperature for 0.5-2 h; the second stage heats to 1400-1600 ℃ at a heating rate of 3-5 ℃/min, and keeps the temperature for 1-3 h.
2. The method of preparing an in situ grown carbon fiber reinforced silicon carbide ceramic matrix composite according to claim 1, wherein the sintering aid comprises SiO 2 、MgO、Al 2 O 3 And Y 2 O 3 Any one or more of the following; the binder comprises polyethylene glycol,Any one or more of ethanol, polyvinyl alcohol, and carboxymethyl cellulose.
3. The method for preparing the in-situ generated carbon fiber reinforced silicon carbide ceramic matrix composite according to claim 2, wherein the mass ratio of the SiC powder to the sintering aid to the binder to the catalyst is as follows: 90-98: 1 to 5:0.5 to 3:1 to 3.
4. The method for preparing an in-situ generated carbon fiber reinforced silicon carbide ceramic matrix composite according to claim 3, wherein the particle size of the SiC powder is 80-120 mesh.
5. The method for preparing an in situ generated carbon fiber reinforced silicon carbide ceramic matrix composite according to claim 1, 2, 3 or 4, wherein the ball milling condition in step 1) is that the ball-to-material ratio is 1: 2-5, the rotating speed is 100-300 r/min, and the ball milling time is 180-300 min.
6. The method for preparing an in situ formed silicon carbide ceramic matrix composite according to claim 5, wherein the molding pressure in step 2) is 80-120 Mpa and the dwell time is 1-5 min.
7. The method for preparing the in-situ generated carbon fiber reinforced silicon carbide ceramic matrix composite according to claim 6, wherein the segmented sintering environment in the step 3) is a vacuum environment, and the vacuum degree is 5-20 Pa.
8. The in-situ formed carbon fiber reinforced silicon carbide ceramic matrix composite material prepared by the preparation method of any one of claims 1 to 7.
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